反应详情

200 ml of water and 300 ml of ethanol were added to 40 g of sodium hydroxide to dissolve the sodium hydroxide. 69.5 g of hydroxylamine hydrochloride was added thereto, and the pH of the solution was adjusted to 10.0 by adding a 2N sodium hydrochloride ethanol/water (3:2) solution mixture. Under cooling with ice, 192 g of ethyl benzoylacetate and a 2N sodium hydroxide in ethanol/water (3:2) solution mixture were added dropwise simultaneously to the reaction solution so that the pH of the reaction solution was 10±0.3. After completion of the addition and stirring for 3 hours at room temperature, the reaction mixture was poured to a mixture of 500 g of concentrated hydrochloric acid and 500 g of ice, then 2.5 liters of ethanol was added to the reaction mixture and after the reaction mixture was heated for 3 hours under reflux, 2 liters of water was added thereto followed by cooling. The precipitated crystals were filtered, washed with water and dried.

1. additionAfter completion of the addition
2. temperatureafter the reaction mixture was heated for 3 hours
3. temperatureunder reflux
4. temperatureby cooling
5. filtrationThe precipitated crystals were filtered
6. washwashed with water
7. customdried